CN219572656U - Carbonization apparatus - Google Patents
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- CN219572656U CN219572656U CN202320344022.4U CN202320344022U CN219572656U CN 219572656 U CN219572656 U CN 219572656U CN 202320344022 U CN202320344022 U CN 202320344022U CN 219572656 U CN219572656 U CN 219572656U
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Abstract
The utility model relates to carbonization equipment, which comprises a carbonization box body, wherein an air inlet channel and an air outlet channel which are oppositely arranged are arranged outside the carbonization box body, and a hollow carbonization cavity group is arranged inside the carbonization box body; and the heat source chamber is used for providing a hot air source, and is communicated with the air inlet channel, so that the hot air source is introduced from the air inlet channel of the carbonization box body, moves in a direction close to the carbonization cavity group and is discharged from the air outlet channel of the carbonization box body. According to the carbonization box, the heat source chamber is arranged outside the carbonization box body, and the heat source in the heat source chamber can enter the hollow carbonization cavity group for carbonization treatment, namely, the carbonization box body does not need to be directly heated, and the heat source with higher temperature can be directly introduced into the carbonization box body, so that the temperature rising rate is higher, the carbonization temperature can be quickly reached in a short time, and the carbonization heating treatment of carbonization equipment is realized.
Description
Technical Field
The utility model belongs to the technical field of high-temperature carbonization, and particularly relates to carbonization equipment.
Background
The existing heat-conducting composite film has the defects of low heat conductivity coefficient and huge difference from theoretical data, researchers are exploring improved methods, and the main improved methods at present are that graphite oxide slurry is optimized, a graphene coating film fragment stacking mode is improved, vacuum carbonization temperature is improved and graphitization temperature is improved, but the performance obtained by the methods is small in improvement amplitude, and the effect is not ideal.
Generally, the heat treatment process in the preparation process of the heat-conductive composite film is roughly divided into three steps: the whole process needs about 30 days for preheating treatment, carbonization and graphitization, wherein a carbonization furnace is usually kept in vacuum in the carbonization process, and a large amount of oxygen-containing functional groups, chlorides, ammonification, tar, trace impurities and the like in the carbon-based film are decomposed and escaped along with the rise of carbonization temperature in the carbonization sintering process, so that a heating material, a heat-insulating material, a furnace wall and the like in a furnace body are subjected to oxidation corrosion and the like, so that the maintenance cost of the furnace body is high, the production cost is high, the performance of the graphene heat-conducting film is improved, the manufacturing cost is reduced, and even the development of the graphene heat-conducting film industry is very unfavorable.
Therefore, it is now highly demanded to develop a carbonization apparatus which is short in process, high in through yield, low in equipment maintenance cost and capable of improving the heat conductive property of the product.
Disclosure of Invention
In order to overcome the defects, the utility model provides the carbonization equipment, which can directly introduce hot gas sources with higher temperature to carry out carbonization treatment without direct heating in the use process, and does not need to set a vacuum environment, so that the carbonization period can be effectively shortened, the energy consumption is obviously reduced, and the service life of the carbonization equipment can be prolonged.
In a first aspect, an embodiment of the present utility model provides a carbonization apparatus, including:
the carbonization device comprises a carbonization box body, wherein an air inlet channel and an air outlet channel which are oppositely arranged are arranged outside the carbonization box body, and a hollow carbonization cavity group is arranged inside the carbonization box body;
and the heat source chamber is used for providing a hot air source, and is communicated with the air inlet channel, so that the hot air source is introduced from the air inlet channel of the carbonization box body, moves in a direction close to the carbonization cavity group and is discharged from the air outlet channel of the carbonization box body.
In some embodiments, the hot gas source is any one of a stream of hot exhaust gas, a stream of hot graphitized volatilized gas, and a stream of hot gas discharged from a carbonization process.
In some embodiments, the intake passage is provided with a first flow regulating valve, and the exhaust passage is provided with a second flow regulating valve.
In some embodiments, the carbonization cavity group comprises a plurality of carbonization cavities arranged at intervals, two adjacent carbonization cavities are communicated with each other, the carbonization cavity group is provided with an unconnected first end and an unconnected second end, the carbonization cavity at the unconnected first end is communicated with the air inlet channel, and the carbonization cavity at the unconnected second end is communicated with the air outlet channel.
In some embodiments, a top of the carbonization cavity is provided with a carbonization cavity cover matched with the carbonization cavity.
In some embodiments, the carbonization cavity of the unconnected first end is further communicated with the channel through a first air flow channel, the first air flow channel is arranged at the top of the carbonization cavity of the unconnected first end, the air inlet channel is arranged at the bottom of the carbonization cavity of the unconnected first end, and a third flow regulating valve is arranged on the first air flow channel; the carbonization cavity of the second end which is not connected is communicated with the exhaust channel through a second airflow channel, the second airflow channel is arranged at the top of the carbonization cavity of the second end which is not connected, the exhaust channel is arranged at the bottom of the carbonization cavity of the second end which is not connected, and a fourth flow regulating valve is arranged on the second airflow channel.
In some embodiments, a carbonization chamber is arranged in the carbonization cavity and is used for accommodating a carbon-based raw material coating film, a carbonization chamber cover matched with the carbonization chamber is arranged on the side wall of the carbonization chamber, and the carbonization chamber is detachably connected with the carbonization chamber cover.
In some embodiments, the top of the carbonization chamber is provided with a hanging ring; and/or
In some embodiments, the bottom of the carbonization chamber is provided with a support frame.
In some embodiments, the top of the carbonization chamber is provided with a one-way valve.
In some embodiments, an exhaust gas treatment device is provided on one side of the carbonization box, and the exhaust gas treatment device is in communication with the exhaust passage.
The technical scheme of the utility model has at least the following beneficial effects:
according to the utility model, the carbonization box body and the heat source chamber are communicated through the air inlet channel, so that a heat source in the heat source chamber can enter the hollow carbonization cavity group for carbonization treatment, namely, the carbonization box body does not need to heat by taking electricity as a heat source, and can directly introduce the heat source with higher temperature into the carbonization box body, the heating rate is higher, the carbonization temperature can be quickly reached in a short time (tens of minutes), and the carbonization heating treatment of the carbonization equipment is realized.
Drawings
The utility model will be further described with reference to the drawings and examples.
FIG. 1 is a schematic perspective view of a carbonization apparatus of the present utility model;
FIG. 2 is a top view of the carbonization device of the present utility model;
FIG. 3 is a front cross-sectional view of a carbonization device of the present utility model;
FIG. 4 is a front view of the carbonization tank of the present utility model.
In the figure:
1-carbonization equipment;
10-carbonizing a box body;
101-a first air flow channel;
102-a second airflow path;
103-a third flow regulating valve;
104-a fourth flow regulating valve;
20-an intake passage;
30-a first flow regulating valve;
40-an exhaust passage;
50-a second flow regulating valve;
60-carbonization cavity;
601-carbonization chamber;
602-carbonization chamber cover;
603-hanging rings;
604-a support frame;
605-one-way valve;
70-carbonizing cavity cover;
80-an exhaust gas treatment device;
90-heat source chamber.
Detailed Description
For a better understanding of the technical solution of the present utility model, the following detailed description of the embodiments of the present utility model refers to the accompanying drawings.
It should be understood that the described embodiments are merely some, but not all, embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The terminology used in the embodiments of the utility model is for the purpose of describing particular embodiments only and is not intended to be limiting of the utility model. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be understood that the term "and/or" as used herein is merely one relationship describing the association of the associated objects, meaning that there may be three relationships, e.g., a and/or B, may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
The existing heat-conducting composite film has the defects of low heat conductivity coefficient and huge difference from theoretical data, and the heat treatment process in the preparation process of the heat-conducting composite film is roughly divided into three steps: preheating treatment, carbonization and graphitization are important links for preparing the heat-conducting composite film, the microstructure and heat-conducting property of the heat-conducting composite film can be greatly influenced, the improvement of the prior art on the carbonization treatment process is usually realized by optimizing the vacuum degree and the temperature in the carbonization furnace, however, the carbonization treatment is carried out by using the carbonization furnace, and the carbonization is realized after the carbonization furnace is slowly heated from room temperature, so that the heating and cooling time in the carbonization treatment process is long, the energy consumption is higher, and the cost is increased; and the carbon-based raw material volatilizes a large amount of impurities such as oxygen-containing functional groups, chlorides, ammonium compounds, tar and the like in the carbonization process, and the impurities corrode equipment such as a thermal insulation graphite felt in a carbonization furnace, the inner wall of the carbonization furnace body, a carbonization furnace pipeline, a carbonization furnace vacuum pump body and the like, so that the service life of the carbonization furnace is greatly reduced.
The applicant researches find that in the carbonization treatment process by adopting the carbonization furnace, the carbonization treatment period is generally 12-36 h, the period is longer, on one hand, the energy consumption is increased, the production cost is increased, and on the other hand, the carbon-based film is heated from room temperature in the carbonization process, so that the internal structure of the carbon-based film is influenced by the relatively slow separation speed of the functional group due to the need of the carbonization furnace, the prepared composite heat-conducting film has structural defects, a perfect six-membered carbon ring structure cannot be formed, a five-membered ring or seven-membered ring structure is easy to form, the integral six-membered carbon ring structure is influenced, and the heat conducting performance of the composite film is lower.
Based on the above-described studies, the present utility model provides a carbonization apparatus 1, referring to fig. 1 to 3, comprising:
the carbonization device comprises a carbonization box body 10, wherein an air inlet channel 20 and an air outlet channel 40 which are oppositely arranged are arranged outside the carbonization box body 10, and a hollow carbonization cavity group is arranged inside the carbonization box body 10;
a heat source chamber 90, the heat source chamber 90 being for providing a hot air source, the heat source chamber 90 being in communication with the air inlet passage 20 such that the hot air source is introduced from the air inlet passage 20 of the carbonization chamber 10, moves in a direction approaching the carbonization chamber group, and is discharged from the air outlet passage 40 of the carbonization chamber 10.
According to the utility model, the carbonization box body 10 and the heat source chamber 90 are arranged and communicated through the air inlet channel 20, so that a heat source in the heat source chamber 90 can enter a hollow carbonization cavity group for carbonization treatment, namely, the carbonization box body 10 of the utility model does not need to heat by taking electricity as a heat source, and can directly introduce a heat source with higher temperature into the carbonization box body 10, so that the heating rate is higher, the carbonization temperature can be quickly reached in a short time (tens of minutes), and the carbonization heating treatment of the carbonization equipment 1 is realized.
In some embodiments, the hot air source is an industrial waste hot air, illustratively any one of a waste hot air stream generated by calcination of minerals, a graphitized volatilized hot gas stream, and a hot gas stream discharged by a carbonization process. In some embodiments, the hot air flow discharged in the carbonization process is the hot air flow generated after carbonization treatment by other carbonization devices such as a carbonization furnace, in other embodiments, the hot air flow discharged in the carbonization process is the hot air flow discharged from the exhaust channel after carbonization treatment by the carbonization device, and the arrangement is such that the hot air source in the carbonization device can be recycled, thereby further reducing energy consumption.
In some embodiments, referring to fig. 1, a first flow rate adjusting valve 30 is disposed on the air inlet channel 20, a second flow rate adjusting valve 50 is disposed on the air outlet channel 40, the first flow rate adjusting valve 30 is used for controlling the flow rate of the hot gas source entering the carbonization tank 10, and the second flow rate adjusting valve 50 is used for controlling the flow rate of the hot gas in the carbonization tank 10.
In some embodiments, referring to fig. 3, the carbonization cavity group includes a plurality of carbonization cavities 60 spaced apart, two adjacent carbonization cavities 60 are communicated with each other, the carbonization cavity group has an unconnected first end and an unconnected second end, the carbonization cavity 60 at the unconnected first end is communicated with the air inlet channel 20, and the carbonization cavity 60 at the unconnected second end is communicated with the air outlet channel 40. In the carbonization device 1, the hot gas source is introduced into the plurality of carbonization cavities 60 which are sequentially communicated through the air inlet channel 20, so that the temperature in the carbonization cavities 60 is quickly increased to the required carbonization temperature and carbonization treatment is carried out, then the hot gas source is discharged from the air outlet channel 40, and in the process of discharging the hot gas source, the flow of the hot gas source in the carbonization cavities 60 can bring impurities such as waste gas generated by carbonization out of the carbonization cavities 60 together, thereby reducing corrosion of the impurities such as waste gas to the carbonization device 1 and being beneficial to prolonging the service life of the carbonization device 1.
In some embodiments, at least 2 carbonization chambers 60 are provided in the carbonization chamber group, specifically, 2, 3, 4, 5, 6, 7, 8, 9 or 10 carbonization chambers may be provided, and in some embodiments, the carbonization chambers 60 are arranged in rows and columns in the carbonization box 10, which is beneficial to improving carbonization efficiency.
In some embodiments, referring to fig. 3, the carbonization cavity 60 at the first end that is not connected is further communicated with the air inlet channel 20 through a first air flow channel 101, the first air flow channel 101 is disposed at the top of the carbonization cavity 60 at the first end that is not connected, the air inlet channel 20 is disposed at the bottom of the carbonization cavity 60 at the first end that is not connected, and a third flow rate adjusting valve 103 is installed on the first air flow channel 101. The carbonization cavity 60 at the second end which is not connected is communicated with the exhaust channel 40 through a second airflow channel 102, the second airflow channel 102 is arranged at the top of the carbonization cavity 60 at the second end which is not connected, the exhaust channel 40 is arranged at the bottom of the carbonization cavity 60 at the second end which is not connected, and a fourth flow regulating valve 104 is arranged on the second airflow channel 102. It will be appreciated that the top and bottom of the carbonization chamber 60 are located opposite, with the top of the carbonization chamber 60 being farther from the bottom of the carbonization chamber 60 than the bottom of the carbonization chamber 60 is from the bottom of the carbonization chamber 60. According to the utility model, the flow rate entering the top of the carbonization cavity 60 is regulated through the third flow regulating valve 103, the gas in the carbonization cavity 60 is prevented from flowing back to the air inlet pipeline, the air flow outside the carbonization device 1 is prevented from entering the carbonization cavity 60, the environment similar to vacuum is formed in the carbonization cavity 60 in the carbonization process, the material to be carbonized in the carbonization device is prevented from being oxidized by hot air, and the carbonization effect of the carbonization cavity 60 is improved. The flow rate exiting the top of the carbonization chamber 60 is regulated by a fourth flow regulating valve 104 to ensure that there is sufficient hot gas source inside the carbonization device 1 to heat the inside of the carbonization device 1.
In some embodiments, referring to fig. 3, a top portion of the carbonization chamber 60 is provided with a carbonization chamber 60 cover that mates with the carbonization chamber 60 to prevent the hot gas source from exhausting outside the carbonization device 1 when circulating in the carbonization chamber 10.
In some embodiments, the steel angle is welded around the carbonization chamber cover 70 as a reinforcing rib, and the carbonization chamber cover 70 and the reinforcing rib are used to facilitate the sealing of the carbonization device 1 during the carbonization treatment.
In some embodiments, the material of the carbonization chamber 60 and/or the carbonization chamber cover 70 comprises at least one of graphite, graphite insulation felt, insulation brick, and refractory insulation ceramic. The carbonization cavity 60 and the carbonization cavity cover 70 made of the above materials can bear high temperature of 1800 ℃, are corrosion-resistant, and can ensure smooth carbonization treatment.
In some embodiments, a thermal insulation material is filled between the carbonization box 10 and the carbonization cavity 60, and the thermal insulation material is a corrosion-resistant material, and the material may specifically be any one of graphite, graphite thermal insulation felt, thermal insulation brick and high-temperature-resistant thermal insulation ceramic.
In some embodiments, referring to fig. 4, a carbonization chamber 601 is disposed in the carbonization cavity 60, where the carbonization chamber 601 is used to accommodate a carbon-based raw material coating film, that is, the carbonization device of the present utility model may be used for carbonization treatment of the carbon-based raw material coating film, and during carbonization treatment, along with the introduction and discharge of a hot air source into the carbonization device, a large amount of oxygen-containing functional groups, chlorides, ammonium compounds, tar, and trace impurities generated during heating of the carbon-based raw material coating film may be discharged from the carbonization device under the driving action of a hot air source flow, so that corrosion of the impurities to the carbonization device may be effectively reduced, and service life of the carbonization device may be prolonged.
Illustratively, the carbonization chamber 601 is of a cuboid structure, the width and depth of the carbonization chamber 601 are 500 mm-1200 mm, 300 mm-500 mm and 1000 mm-2500 mm respectively, the side part of the carbonization chamber 601 is provided with a carbonization chamber cover 602 matched with the carbonization chamber 601, and the carbonization chamber 601 is detachably connected with the carbonization chamber cover 602. Before carbonization treatment, the carbon-based raw material coating film is placed in a carbonization chamber 601, a carbonization chamber cover 602 is covered, the carbonization chamber 601 loaded with the carbon-based raw material coating film is placed in a carbonization cavity 60, a carbonization cavity cover 70 is covered, a hot air source is introduced, the hot air source circulates in an air flow channel and conducts heat transfer and heating to the carbonization chamber 601, and therefore heating carbonization treatment of the carbon-based raw material coating film in the carbonization chamber 601 is achieved.
In some embodiments, 20 to 100 locking points are arranged around the carbonization chamber cover 602, the carbonization chamber cover 602 is connected with the carbonization chamber 601 through at least one of flange holes, buckles, slots and chucks, and thus, the sealing effect between the carbonization chamber 601 and the carbonization chamber cover 602 can be ensured, and external gas is prevented from entering the carbonization chamber 601 in the carbonization process.
In some embodiments, the material of the carbonization chamber 601 and/or the carbonization chamber cover 602 is any one of stainless steel and graphite.
In some embodiments, referring still to fig. 4, a top portion of the carbonization chamber 601 is provided with a hanging ring 603. The hanging ring 603 is arranged to facilitate the taking of the carbonization chamber 601, and illustratively, the hanging ring 603 is made of one of 304 stainless steel, graphite and carbon steel, so that the strength requirement of the carbonization box 10 can be ensured.
In some embodiments, referring still to FIG. 4, a support frame 604 is provided at the bottom of the carbonization chamber 601. The carbonization chamber 601 is placed in the carbonization cavity 60 through the support frame 604, which is favorable for good heat transfer at the bottom of the carbonization chamber 601, and the support frame 604 is made of stainless steel for example.
In some embodiments, referring to fig. 4, a check valve 605 is disposed at the top of the carbonization chamber 601, and the check valve 605 is used to enable the gas inside the carbonization chamber 601 to be exhausted unidirectionally, and prevent the external air from entering the carbonization chamber 601, so as to avoid pollution of the carbon-based raw material coating film in the carbonization chamber 601.
In summary, the structure of the carbonization chamber 601 of the present utility model can ensure that the inside of the carbonization chamber 601 achieves the vacuum effect of the vacuum carbonization furnace, and ensure that the carbon-based raw material coating film is not oxidized in the carbonization process, thereby realizing a high-efficiency and low-cost carbonization process.
In some embodiments, referring still to FIG. 3, an exhaust treatment device 80 is provided on one side of the carbonization box 10, the exhaust treatment device 80 being in communication with the exhaust passage 40. The exhaust gas treatment device 80 is provided to treat the exhaust gas discharged from the exhaust passage 40, thereby avoiding pollution to the environment. It is to be understood that the exhaust treatment device 80 of the present utility model is a commercially available exhaust treatment device or purification device that is conventional in the art, and the present utility model is not limited to the particular type of exhaust treatment device 80.
The utility model also provides a preparation process for preparing the composite film by adopting the carbonization equipment, which comprises the following steps:
placing the carbon-based raw material coating film in the carbonization equipment, introducing a hot gas source in a heat source chamber from an air inlet channel, moving in a direction close to the carbon-based raw material coating film, and discharging the hot gas from an air outlet channel, so that the carbonization equipment heats up to 600-1500 ℃ at a heating rate of 10-100 ℃/min, and carbonizing the carbon-based raw material coating film to obtain a first precursor;
and graphitizing the first precursor to obtain the composite film.
In the preparation method of the composite film, the carbon-based raw material coating film is heated by the hot air source introduced into the carbonization equipment, a carbonization furnace is not needed to be used for heating from room temperature, the heating rate is high, the carbonization temperature can be quickly reached in a short time (tens of minutes), and the energy consumption is reduced while the carbonization treatment temperature is ensured; in addition, as a hot air source is introduced and discharged into the carbonization equipment, a large amount of oxygen-containing functional groups, chlorides, ammonium compounds, tar, trace impurities and the like generated in the heating process of the carbon-based raw material coating film can be discharged out of the carbonization equipment under the driving action of hot air source air flow, so that the corrosion of the impurities to the carbonization equipment can be effectively reduced, the service life of the carbonization equipment is prolonged, in addition, in the hot air flow process, the hot air flow conducts heat to the carbonization equipment, so that the carbonization equipment heats up to 600-1500 ℃ at the heating rate of 10-100 ℃/min to carbonize the carbon-based raw material coating film.
According to the preparation method disclosed by the utility model, the carbonization treatment does not need to be operated in a vacuum environment, so that the preparation cost can be effectively reduced, the energy consumption can be reduced, the process efficiency can be improved, and the production efficiency can be improved.
The specific preparation method of the composite film according to the present utility model is described in further detail below.
Step S100, preparing sizing agent of the carbon-based raw material coating film.
In some embodiments, the carbon-based raw material coating film includes at least one of a graphene coating film, a graphite-based coating film, a carbon nanotube coating film, and an organic polymer film. The graphite-based coating film may be an artificial graphite coating film or an artificial graphite-like coating film, and the artificial graphite-like coating film may be a super-crystalline graphite coating film, for example. The organic polymer film includes at least one of a polyimide film (PI film) and a polyoxadiazole fiber film (POD film).
Taking the slurry for preparing the graphene coating film as an example, the preparation method comprises the following steps: dissolving graphite oxide in ultrapure water, adding alkaline substances, and preparing graphene oxide slurry with the solid content of 0.1% -10% through three dispersing procedures of stirring, homogenizing and defoaming.
In some embodiments, the viscosity value of the graphene oxide slurry may be 10000cps to 80000cps, specifically 10000cps, 20000cps, 30000cps, 40000cps, 50000cps, 60000cps, 70000cps, or 80000cps, or the like, but may be other values within the above range, which is not limited thereto.
In some embodiments, the pH of the graphene oxide slurry is 5 to 9, specifically 5, 6, 7, 8 or 9, or the like, but other values within the above range are also possible, and the present utility model is not limited thereto.
In some embodiments, the basic substance comprises at least one of an inorganic base comprising at least one of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, ammonium carbonate, and calcium hydroxide, and an organic base comprising at least one of methylamine, ethylamine, methanol amine, ethanolamine, and triethanolamine.
In some embodiments, the stirring process may specifically be: dispersing for 10 min-30 min at 500-1000 rpm in a stirrer, and dispersing for 30 min-120 min at 2000-5000 rpm.
In some embodiments, the homogenizing process may specifically be: homogenizing in a homogenizer at 20-60 bar for the first time, at 40-100 bar for the second time, and at 60-120 bar for the third time.
In some embodiments, the defoaming procedure may specifically be: the operation is carried out once in a rotary deaeration machine at a rotation speed of 600 rpm-1200 rpm and a vacuum degree of-0.1 MPa. It will be appreciated that the material flow from the mixer to the homogenizer to the deaerator is through an automated slurry feed system.
Step S200, coating the slurry obtained in step S100 to obtain a carbon-based raw material coating film.
Specific: and (3) inputting the slurry obtained in the step (S100) into a trough of a coating machine through an automatic feeding system, uniformly coating the slurry on a carrier through a slit with a preset thickness, then, primarily drying in a baking oven of the coating machine, winding at the tail of the coating machine to obtain a carbon-based raw material coating film coiled material, and finally, cutting the carbon-based raw material coating film coiled material into a specific size to obtain the carbon-based raw material coating film.
In some embodiments, the thickness of the slit to be coated is 0.5mm to 10mm, specifically, may be 0.5mm, 1mm, 3mm, 5mm, 7mm, 8mm, or 10mm, etc., but may be other values within the above range, and is not limited thereto.
In some embodiments, the coating carrier is a double-sided breathable special material filter cloth, and the material of the coating carrier includes, but is not limited to, at least one of terylene, polypropylene, nylon-6 and polytetrafluoroethylene, and is acid and alkali resistant.
In some embodiments, the coated support has a gas permeability of 5L/m 2 ·s～200L/m 2 S, which may be in particular 5L/m 2 ·s、10L/m 2 ·s、20L/m 2 ·s、5L/m 2 ·s、70L/m 2 ·s、100L/m 2 ·s、150L/m 2 S and 200L/m 2 S, etc., may be any other value within the above range, and is not limited thereto.
In some embodiments, the weave of the coated carrier is at least one of satin and twill.
In some embodiments, the coated carrier structure comprises at least one of a monofilament, a multifilament, and a multifilament.
In some embodiments, the drying temperature is 50 to 100 ℃, specifically 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃ and the like, but may be any other value within the above range, and the drying temperature is not limited thereto.
It will be appreciated that steps S100 to S200 may be omitted, and that the carbon-based raw material coating film purchased or already prepared may be directly selected as a raw material.
Step S300, preheating the carbon-based raw material coating film.
In some embodiments, the temperature of the preheating treatment is 80 to 200 ℃, specifically, the temperature of the preheating treatment may be, for example, 80 ℃, 100 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, or 200 ℃, or the like, but may be any other value within the above range, and the temperature is not limited thereto. The preheating treatment temperature is controlled at 80-200 ℃, so that on one hand, the effect of drying the carbon-based raw material coating film can be achieved, and on the other hand, the moisture (non-crystal water) in the carbon-based raw material coating film is slowly released, so that the compactness between fragments inside the carbon-based material is improved, the cohesive force of the carbon-based material film is enhanced, and the interlayer binding force of the carbon-based material is improved. If the temperature of the preheating treatment is higher than 200 ℃, the carbon-based raw material coating film is easy to excessively expand and even crack into fragments, the internal interlayer structure of the obtained composite film is fluffy, and the interlayer bonding force is weak and easy to peel after calendaring.
In some embodiments, the heating rate of the preheating treatment is 0.05 to 5 ℃ per minute, specifically, 0.05, 0.1, 0.3, 0.8, 1, 2, 3, 4, or 5 ℃ per minute, but other values within the above range are also possible, and the method is not limited thereto. The heating rate is greater than 5 ℃/min, so that the moisture in the carbon-based raw material coating film is rapidly converted into steam, the carbon-based raw material coating film is easy to excessively expand, even the cracking film is broken into pieces, and the binding force of the film layer is reduced. The temperature rising rate is less than 0.05 ℃/min, which results in the reduction of the process efficiency and the increase of the production cost.
In some embodiments, the preheating treatment time is 30min to 300min, specifically, 30min, 60min, 120min, 150min, 180min, 240min, or 300min, or the like, but other values within the above range are also possible, and the method is not limited thereto.
In some embodiments, the apparatus for the preheating treatment includes at least one of a drying oven and an oven.
And step S400, placing the carbon-based raw material coating film obtained in the step S300 into carbonization equipment, introducing a hot air source from an air inlet channel of the carbonization equipment, moving towards a direction close to the carbon-based raw material coating film, and discharging from an air outlet channel of the carbonization equipment, so that the carbonization equipment is heated to 600-1500 ℃ at a heating rate of 10-100 ℃/min, and carbonizing the carbon-based raw material coating film to obtain a first precursor.
In some embodiments, the hot gas source comprises at least one of a stream of hot exhaust gas, a stream of graphitized volatilized hot gas, and a stream of hot gas discharged from a carbonization process.
In some embodiments, the flow rate of the hot gas source is 0.5m 3 /min～5m 3 Each of the values/min may be 0.5m 3 /min、0.8m 3 /min、1m 3 /min、2m 3 /min、3m 3 /min、4m 3 /min or 5m 3 However, the value of the ratio may be other values within the above range, and the ratio is not limited thereto.
In some embodiments, the temperature of the carbonization treatment is 600 ℃ to 1500 ℃, specifically, the temperature of the carbonization treatment may be 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃, or the like, but may be other values within the above range, and the present utility model is not limited thereto.
In some embodiments, the hot gas source is directly introduced into the carbonization equipment, the temperature of the hot gas source is higher, the rapid temperature rise inside the carbonization equipment can be realized, the temperature rise rate can reach 10 ℃/min-100 ℃/min, the specific temperature rise rate can be 10 ℃/min, 20 ℃/min, 30 ℃/min, 40 ℃/min, 50 ℃/min, 60 ℃/min, 70 ℃/min, 80 ℃/min, 90 ℃/min or 100 ℃/min, and the like, and other values in the range can be certainly adopted, and the utility model is not limited. Preferably, the heating rate is 20 ℃/min to 40 ℃/min. Compared with the prior art that carbonization treatment needs to slowly raise the temperature in a vacuum atmosphere (the common heating rate is 1 ℃/min-3 ℃/min), the utility model has the advantages that the time for reaching the carbonization temperature in carbonization equipment is shorter, the time for raising the temperature to the carbonization treatment temperature is 10-20 min, the energy consumption can be reduced, the working efficiency can be improved, and the thermal performance of the composite film can be effectively improved.
It will be appreciated that the carbonization temperature and temperature rise rate data of the carbonization treatment of the present utility model are obtained by measuring the data in the carbonization chamber 101.
In some embodiments, the holding time of the carbonization treatment is 2h to 6h, specifically, may be 2h, 3h, 4h, 5h, 6h, or the like, and of course, may be other values within the above range, and is not limited thereto.
Step S500, graphitizing the first precursor.
In some embodiments, the temperature rise rate of the graphitization treatment is 0.2 ℃/min to 1.5 ℃/min, specifically, 0.2 ℃/min, 0.5 ℃/min, 0.8 ℃/min, 1.0 ℃/min, 1.2 ℃/min, 1.5 ℃/min, etc., but may be other values within the above range, and the utility model is not limited thereto.
In some embodiments, the graphitization treatment temperature is 2400 to 3200 ℃, specifically 2400 to 2500 ℃, 2600 ℃, 2700 ℃, 2800 ℃, 2900 ℃, 3000 ℃, 3100 ℃, 3200 ℃ or the like, but other values within the above range are also possible, and the graphitization treatment temperature is not limited thereto.
In some embodiments, the heat preservation time of the graphitization treatment is 60min to 900min, specifically, 60min, 90min, 120min, 150min, 180min, 300min, 400min, 500min, 600min, 700min, 800min or 900min, or the like, but other values within the above range are also possible, and the method is not limited thereto.
In some embodiments, the graphitizing apparatus comprises at least one of an acheson graphitizing furnace, a van graphitizing furnace, a continuous graphitizing furnace, and an in-line graphitizing furnace.
In some embodiments, the graphitizing treatment is performed in a protective gas atmosphere comprising at least one of nitrogen, argon, neon, and xenon.
Step S600, after graphitizing, calendaring the graphitized material.
In some embodiments, the calendering process includes at least one of vacuum platen pressing, vacuum roll pressing, non-vacuum platen pressing, and non-vacuum roll pressing.
In some embodiments, the vacuum degree of the rolling treatment is-0.1 MPa to-0.05 MPa, specifically, the vacuum degree of the rolling treatment may be-0.1 MPa, -0.09MPa, -0.08MPa, -0.07MPa, -0.06MPa or-0.05 MPa, etc., of course, other values within the above range are also possible, and the present utility model is not limited thereto.
In some embodiments, the pressure of the rolling treatment is 5MPa to 100MPa, specifically, 5MPa, 10MPa, 20MPa, 30MPa, 50MPa, 70MPa, 80MPa, 100MPa, or the like, but other values within the above range are also possible, and the rolling treatment is not limited thereto.
In some embodiments, the present utility model also provides a composite film prepared by the above-described preparation method, the composite film comprising carbon-based materials arranged in a stack, in the raman spectrum of the composite film, I D /I G ≤0.01，I D Representing the D peak at a wavelength of 1300cm -1 Strength at point I G Representing the G peak at a wavelength of 1580cm -1 Is a strength of (a) is a strength of (b). Specifically, I D /I G The values may be 0.001, 0.003, 0.005, 0.008, 0.01, or the like, but other values within the above range are also possible, and the present utility model is not limited thereto. Within the above range, it is shown that the composite film of the present utility model is I D /I G The composite membrane carbon-based material has smaller internal crystallization, which is beneficial to forming a perfect six-membered carbocycle structure and improving the heat conduction performance of the composite membrane.
In some embodiments, the carbon-based material comprises one of graphene, graphite, and carbon nanotubes.
In some embodiments, the grain size L of the carbon-based material c 95nm or more, specifically, the grain size L of the carbon-based material c The wavelength may be 95nm, 96nm, 97nm, 98nm or 99nm, or other values within the above range, and the present utility model is not limited thereto. The crystal grain size of the carbon-based material is larger, which indicates that the heat conductivity coefficient of the composite film is higher.
In some embodiments, the interplanar spacing d002 of the carbon-based material is 0.3380 or less, specifically, the interplanar spacing d002 of the carbon-based material may be, for example, 0.3354, 0.3355, 0.3356, 0.3360, 0.3370, or 0.3380, or the like, but other values within the above range are also possible, and the present utility model is not limited thereto. The carbon-based material has smaller interplanar spacing, which indicates that the graphitization degree of the composite film is higher, and the heat conductivity coefficient of the composite film can be improved.
In some embodiments, the thermal conductivity of the composite film is 1300W/mK to 2100W/mK, specifically 1300W/mK, 1400W/mK, 1500W/mK, 1600W/mK, 1700W/mK, 1800W/mK, 1900W/mK, 2000W/mK, 2100W/mK, etc., but other values within the above range are also possible, and the utility model is not limited thereto.
In some embodiments, the thermal diffusivity of the composite film is 720mm 2 /s～1100mm 2 S, which may be 720mm 2 /s、730mm 2 /s、740mm 2 /s、750mm 2 /s、800mm 2 /s、900mm 2 /s、1000mm 2 /s or 1100mm 2 Of course, other values within the above range are also possible, and the present utility model is not limited thereto.
In some embodiments, the composite film has a density of 1.7g/cm 3 ～2.2g/cm 3 Specifically, it may be 1.7g/cm 3 、1.8g/cm 3 、1.9g/cm 3 、2.0g/cm 3 、2.1g/cm 3 Or 2.2g/cm 3 And the like, but of course, other values within the above range are also possible, and are not limited thereto.
In some embodiments, the degree of graphitization of the composite film is 99% or more, and the degree of graphitization of the composite film may be specifically 99%, 99.1%, 99.2%, 99.5%, 99.7%, 99.9%, or the like, but may be other values within the above range, and is not limited thereto.
In some embodiments, the fixed carbon content of the composite membrane is greater than 99.5%.
Example 1
(1) And (3) coating, drying and forming a film from graphene oxide composite slurry with the solid content of 6wt%, preheating at 200 ℃ for 5 hours to obtain a reduced graphene oxide film, cutting the reduced graphene oxide film, and loading the cut reduced graphene oxide film into a carbonization box.
(2) Placing the carbonization box with the reduced graphene oxide film into a carbonization cavity of carbonization equipment, the carbonization equipment is heated and carbonized by adopting waste gas hot air flow generated by the calcination of minerals in a heat source chamber, so that the carbonization equipment is heated to 1200 ℃ according to the heating rate of 20 ℃/min, and is kept for 4 hours, and the carbonization equipment is characterized in thatIn which the flow rate of the hot air flow of the exhaust gas is 3m 3 /min。
(3) And (3) loading the carbonized graphene film into a high-temperature graphitization furnace, heating to 3000 ℃ according to the heating rate of 0.8 ℃/min, and preserving heat for 10 hours to prepare the graphene fluffy film.
(4) And (3) rolling the graphene fluffy film obtained in the step (3) under the pressure of 6MPa to prepare the graphene film.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 2
Unlike example 1, the carbonization temperature of step (2) was 600 ℃.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 3
Unlike example 1, the carbonization temperature of step (2) was 1000 ℃.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 4
Unlike example 1, the carbonization temperature of step (2) was 1500 ℃.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 5
Unlike example 1, the flow rate or flow rate of the exhaust hot air stream in step (2) was 0.5m 3 /min。
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 6
Unlike example 1, the flow rate or flow rate of the exhaust hot air stream in step (2) was 5m 3 /min。
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 7
Unlike example 1, the holding time for carbonization in step (2) was 2 hours.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 8
Unlike example 1, the incubation time for carbonization in step (2) was 6h.
The composite film of this embodiment includes graphene arranged in a stacked manner, and the performance parameters of the composite film are shown in table 1.
Example 9
Unlike example 1, the temperature rise rate of the carbonization device in step (2) was 10℃per minute, and the flow rate of the exhaust hot air stream was 1m 3 /min。
Example 10
Unlike example 1, the heating rate of the carbonization device in step (2) was 40℃per minute, and the flow rate of the exhaust hot air stream was 5m 3 /min。
Example 11
Unlike example 1, the temperature rise rate of the carbonization device in step (2) was 50℃per minute, and the flow rate of the exhaust hot air stream was 3m 3 /min。
Example 12
Unlike example 1, the heating rate of the carbonization device in step (2) was 100℃per minute, and the flow rate of the exhaust hot air stream was 5m 3 /min。
Comparative example 1
Unlike example 1, the carbonization treatment was performed in step (2) using a conventional vacuum carbonization furnace, the heating rate of the carbonization treatment was 1 ℃/min, the carbonization temperature was 1200 ℃, and the heat-retaining time of the carbonization treatment was 4 hours.
Performance testing
1. Thermal conductivity testing: the equipment is LFA-467Hyper Flash; the thermal diffusivity was measured by cutting a sample into a 25.4mm diameter disc, with reference to ASTM-E1461, standard test method for fixed thermal conductivity by flash method. Thermal conductivity = thermal diffusivity × density × specific heat capacity calculation. (specific heat capacity: 0.85).
2. Degree of graphitization: characteristic peaks were obtained by XRD diffraction testThe graphite layer spacing was calculated by bragg diffraction equation d002=nλ/2sin θ (n=1, λ= 0.15406), by p= (0.3440-d) 002 ) Calculating the graphitization degree according to the ratio of (0.3440-0.3354);
3. lc grain size: characteristic peaks were obtained by XRD diffractometry, and the grain size was calculated by Scherrer formula lc=kλ/βcosθ (k=0.9, λ= 0.15406).
4. The raman spectrum is tested using an xpora full-automatic raman spectrometer by: excitation wavelength 532nm, power 1mW, scanning wave number range 500cm -1 ～4000cm -1 . Peak intensities were calculated using gaussian fitting of G and D peaks.
Examples 1 to 8 and comparative example 1 were tested in the manner described above, and the results are shown in table 1.
TABLE 1 Performance parameters of the composite films prepared in examples and comparative examples
As can be seen from the data in table 1: the composite film is prepared by the carbonization equipment, the temperature rising rate of the carbonization equipment is high, the carbonization temperature can be quickly reached in a short time (tens of minutes), and the energy consumption is reduced while the carbonization treatment temperature is ensured; in addition, along with the introduction and discharge of a hot air source in the carbonization equipment, a large amount of oxygen-containing functional groups, chlorides, ammonium compounds, tar, trace impurities and the like generated in the heating process of the carbon-based raw material coating film can be discharged out of the carbonization equipment under the driving action of hot air source air flow, so that the corrosion of the impurities to the carbonization equipment can be effectively reduced, and the service life of the carbonization equipment is prolonged. The carbonization treatment is carried out on the carbon-based raw material coating film by the carbonization equipment, so that the temperature of the carbon-based raw material coating film is raised to the carbonization temperature, and the Yu Tanji raw material composite film is favorably rearranged to form a perfect six-membered ring structure in the carbonization process, thereby improving the heat conduction performance of the composite film.
In comparative example 1, the conventional carbonization furnace is adopted for carbonization treatment, and the temperature needs to be raised from room temperature, so that the carbonization time is longer, the internal consumption and the cost are increased, and the heat conduction performance of the prepared composite film is also reduced; moreover, because the inside of the carbonization furnace needs vacuumizing treatment, impurities generated by the carbon-based raw material coating film under the heating condition are applied to equipment such as a heat-insulation graphite felt in the carbonization furnace, the inner wall of the carbonization furnace, a carbonization furnace pipeline, a carbonization furnace vacuum pump body and the like, so that the service life of the carbonization furnace is greatly reduced.
While the above description of a carbonization device provided by the present utility model has been provided in detail, specific examples are employed herein to illustrate the principles and embodiments of the present utility model, and the above examples are provided only to assist in understanding the method of the present utility model and its core ideas; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present utility model, the present description should not be construed as limiting the present utility model in view of the above.
Claims (10)
1. A carbonization device, comprising:
the carbonization device comprises a carbonization box body, wherein an air inlet channel and an air outlet channel which are oppositely arranged are arranged outside the carbonization box body, and a hollow carbonization cavity group is arranged inside the carbonization box body;
and the heat source chamber is used for providing a hot air source, and is communicated with the air inlet channel, so that the hot air source is introduced from the air inlet channel of the carbonization box body, moves in a direction close to the carbonization cavity group and is discharged from the air outlet channel of the carbonization box body.
2. The carbonization device as claimed in claim 1, wherein the hot air source is industrial waste hot air.
3. The carbonization device according to claim 1, wherein a first flow rate adjustment valve is provided on the intake passage, and a second flow rate adjustment valve is provided on the exhaust passage.
4. The carbonization device according to claim 1, wherein the carbonization cavity group comprises a plurality of carbonization cavities arranged at intervals, two adjacent carbonization cavities are communicated with each other, the carbonization cavity group has an unconnected first end and an unconnected second end, the carbonization cavity at the unconnected first end is communicated with the air inlet channel, and the carbonization cavity at the unconnected second end is communicated with the air outlet channel.
5. The carbonization device as claimed in claim 4, wherein a top of the carbonization chamber is provided with a carbonization chamber cover cooperating with the carbonization chamber.
6. The carbonization device according to claim 4, wherein the carbonization cavity of the unconnected first end is further communicated with the channel through a first air flow channel, the first air flow channel is arranged at the top of the carbonization cavity of the unconnected first end, the air inlet channel is arranged at the bottom of the carbonization cavity of the unconnected first end, and a third flow rate regulating valve is arranged on the first air flow channel; the carbonization cavity of the second end which is not connected is communicated with the exhaust channel through a second airflow channel, the second airflow channel is arranged at the top of the carbonization cavity of the second end which is not connected, the exhaust channel is arranged at the bottom of the carbonization cavity of the second end which is not connected, and a fourth flow regulating valve is arranged on the second airflow channel.
7. The carbonization device according to claim 4, wherein a carbonization chamber is provided in the carbonization chamber for accommodating the carbon-based raw material coating film, a carbonization chamber cover is provided on a side wall of the carbonization chamber to be matched with the carbonization chamber, and the carbonization chamber is detachably connected with the carbonization chamber cover.
8. The carbonization device as claimed in claim 7, wherein a hanging ring is provided at the top of the carbonization chamber; and/or
The bottom of the carbonization chamber is provided with a supporting frame.
9. The carbonization device as claimed in claim 7, wherein a top of the carbonization chamber is provided with a one-way valve.
10. The carbonization device as claimed in claim 1, wherein an exhaust gas treatment device is provided at one side of the carbonization tank, and the exhaust gas treatment device is communicated with the exhaust passage.
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